Acetic Acid → HCID 70031142, 화합물

HRID 397534노트

반응식

HRID 397534 반응식
[NH2:1][C:2]1[C:3]([F:14])=[C:4]([CH2:9][C:10]([O:12][CH3:13])=[O:11])[C:5]([F:8])=[CH:6][CH:7]=1.CC(O)=O.[CH:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=1)=[CH2:20]>CO>[N:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[CH2:19][CH2:20][NH:1][C:2]1[C:3]([F:14])=[C:4]([CH2:9][C:10]([O:12][CH3:13])=[O:11])[C:5]([F:8])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 75212-VinylpyridineHCID 10965547Methyl 2-(3-amino-2,6-difluorophenyl)acetate

생성물 1

HCID 70031142HCID 70031142, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 402 mg (2.0 mmol) of methyl 3-amino-2,6-difluorophenylacetate (prepared in step 3 of example 24) in 15 mL of MeOH was treated with 1.1 mL (20.0 mmol) of HOAc and 0.28 mL (2.6 mmol) of 2-vinylpyridine. The reaction mixture was stirred at reflux for 16 h. The mixture was cooled and the acetic acid was removed in vacuo. The residue was dissolved in EtOAc and washed with saturated NaHCO3 (4×5 mL), water (1×10 mL) and brine. Column chromatography (1:4 EtOAc/Hex) afforded methyl 3-(2-pyridylethyl)amino-2,6-difluorophenylacetate.

후처리

  1. temperatureat reflux for 16 h
  2. temperatureThe mixture was cooled
  3. customthe acetic acid was removed in vacuo
  4. dissolutionThe residue was dissolved in EtOAc
  5. washwashed with saturated NaHCO3 (4×5 mL), water (1×10 mL) and brine

출처 및 근거

ORD 기록
ord-d57aae8940ad42a39594f288979475f2
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610701B2

반응 노트

불러오는 중…